Electrospray ionization mass spectrometry and partial least squares discriminant analysis applied to the quality control of olive oil

Direct infusion electrospray ionization mass spectrometry in the positive ion mode [ESI(+)‐MS] is used to obtain fingerprints of aqueous–methanolic extracts of two types of olive oils, extra virgin (EV) and ordinary (OR), as well as of samples of EV olive oil adulterated by the addition of OR olive oil and other edible oils: corn (CO), sunflower (SF), soybean (SO) and canola (CA). The MS data is treated by the partial least squares discriminant analysis (PLS‐DA) protocol aiming at discriminating the above‐mentioned classes formed by the genuine olive oils, EV (1) and OR (2), as well as the EV adulterated samples, i.e. EV/SO (3), EV/CO (4), EV/SF (5), EV/CA (6) and EV/OR (7). The PLS‐DA model employed is built with 190 and 70 samples for the training and test sets, respectively. For all classes (1–7), EV and OR olive oils as well as the adulterated samples (in a proportion varying from 0.5 to 20.0% w/w) are properly classified. The developed methodology required no ions identification and demonstrated to be fast, as each measurement lasted about 3 min including the extraction step and MS analysis, and reliable, because high sensitivities (rate of true positives) and specificities (rate of true negatives) were achieved. Finally, it can be envisaged that this approach has potential to be applied in quality control of EV olive oils. Copyright © 2013 John Wiley & Sons, Ltd.     

Pulsed Nd:YAG laser welding of AISI 304 to AISI 420 stainless steels

The technique to weld AISI 304 stainless steel to AISI 420 stainless steel with a pulsed Nd:YAG laser has been investigated. The main objective of this study was to determine the influence of the laser beam position, with respect to the joint, on weld characteristics. Specimens were welded with the laser beam incident on the joint and moved 0.1 and 0.2 mm on either side of the joint. The joints were examined in an optical microscope for cracks, pores and to determine the weld geometry. The microstructure of the weld and the heat affected zones were observed in a scanning electron microscope. An energy dispersive spectrometer, coupled to the scanning electron microscope, was used to determine variations in (weight %) the main chemical elements across the fillet weld. Vickers microhardness testing and tensile testing were carried out to determine the mechanical properties of the weld. The results of the various tests and examinations enabled definition of the best position for the incident laser beam with respect to the joint, for welding together the two stainless steels.     

Ion synthesis and optical properties of gold nanoparticles in an Al2O3 matrix

Single-crystal Al₂O₃(0001) and Al₂O₃(1120) substrates are implanted by 160-keV Au⁺ ions with doses from 10¹⁵ to 10¹⁷ cm^?2. Some of the implanted samples are air-annealed at 800–1200°C. The properties of the synthesized composite layers are studied by Rutherford backscattering and linear optical reflection measurements, and their nonlinear optical characteristics are examined by RZ-scanning using a picosecond Nd: YAG laser operating at a wavelength of 1064 nm. The Rutherford backscattering spectra indicate that the implanted impurity concentrates near the surface of the Al₂O₃. The formation of gold nanoparticles in the Al₂O₃ can be judged from the characteristic optical plasmon resonance band in the reflectance spectra of the samples irradiated to a dose higher than 6.0 × 10¹⁶ cm^?2. The synthesized particles are shown to be responsible for nonlinear optical refraction in the samples. The nonlinear refractive index, n ₂, and the real part of the third-order susceptibility, Rex⁽³⁾, of the composite layers are determined.     

The structure of crystallographic damage in GaN formed during rare earth ion implantation with and without an ultrathin AlN capping layer

The crystallographic nature of the damage created in GaN implanted by rare earth ions at 300 keV and room temperature has been investigated by transmission electron microscopy versus the fluence, from 7×10¹³ to 2×10¹⁶ at/cm², using Er, Eu or Tm ions. The density of point defect clusters was seen to increase with the fluence. From about 3×10¹⁵ at/cm², a highly disordered ‘nanocrystalline layer’ (NL) appears on the GaN surface. Its structure exhibits a mixture of voids and misoriented nanocrystallites. Basal stacking faults (BSFs) of I₁, E and I₂ types have been noticed from the lowest fluence, they are I₁ in the majority. Their density increases and saturates when the NL is observed. Many prismatic stacking faults (PSFs) with Drum atomic configuration have been identified. The I₁ BSFs are shown to propagate easily through GaN by folding from basal to prismatic planes thanks to the PSFs.When implanting through a 10 nm AlN cap, the NL threshold goes up to about 3×10¹⁶ at/cm². The AlN cap plays a protective role against the dissociation of the GaN up to the highest fluences. The flat surface after implantation and the absence of SFs in the AlN cap indicate its high resistance to the damage formation.     

Optical studies of ZnO nanocrystals doped with Eu3+ ions

Synthetic ZnO nanocrystals have been intentionally doped with Eu³⁺ ions. Structural analysis performed on the nanocrystals showed wurtzite-ZnO as the only phase present in the samples. Photoluminescence in emission and excitation modes allows the assignment of the intra-4f⁶ transitions for the Eu³⁺ ions. From the analysis of the optical data we are able to demonstrate that multiple Eu-related optical centres are present in the studied samples. Oxygen vacancies are likely candidates to be responsible for the ion accommodation in the ZnO lattice and from the photoluminescence excitation data we tentatively assign a trap level at ∼200 meV below the conduction band to this intrinsic defect. PACS 78.66.Hf; 78.67.-n; 82.80.Yc     

Nanostructures of sodium titanate/zirconium oxide

In this work is reported the synthesis of nanotubes and nanoribbons from mixed oxides (Ti_1−x Zr _x O₂·nH₂O), employing hydrothermal treatment in a highly alkaline medium. The morphology and crystal structure of the products obtained via hydrothermal treatment depend on the value of x. For example, for x equal to 0 and 0.50 were observed the presence of nanotubes (diameter around 9 nm) and nanoribbons (diameter around 200 nm), respectively. However, for x values above 0.50, there was no morphological change. Regarding the crystalline structure of these samples, for x equal to 0 was observed the sodium titanate phase; already for x values up to 0.50, we observed the presence of two crystalline phases: sodium titanate and tetragonal ZrO₂. For x values above 0.50, only tetragonal ZrO₂ was observed. Furthermore, only the product obtained from x equal to 0.15 was observed the presence of three-dimensional flower-like arrangements. The results obtained by the characterization techniques showed the segregation of zirconium after hydrothermal treatment of precursors with x less or equal to 0.50. Thus, we describe the important role that Ti/Zr molar ratio of the precursor plays on the morphology and crystalline phase of the products formed by hydrothermal treatment.     

Disposable pipette tips extraction: Fundamentals,applications and state of the art

Disposable pipette tips extraction consists of a solid‐phase extraction in which the sorbent is poorly dispersed in a pipette tip, which allows a quick and dynamic contact between the aspirated analyte from the sample and the solid phase. It is a technique used particularly in food and forensic analysis, since it requires a small amount of sample and solvent. This article highlights the principles, advantages and disadvantages of the disposable pipette tips extraction method and reviews recent applications.     

Diastereo-controlled Diels–Alder cycloadditions of erythrose benzylidene-acetal 1,3-butadienes by 4-substituted-1,2,4-triazoline-3,5-dione: Evidence for the stereoelectronic effects on the dienes

Erythrose benzylidene-acetal 1,3-butadienes are studied as partners in Diels–Alder cycloadditions. A high diastereofacial improvement is found in cases where both the alcohol function is protected and a π–π interaction between the diene and dienophile is possible. Several competing factors have been studied independently in order to explain its influence on the selectivity of the cycloadditions.     

Structure characterization and mechanism of growth of PbTe nanocrystals embedded in a silicate glass

A nanocomposite consisting of PbTe nanocrystals embedded in a silicate glass was studied by small-angle x-ray scattering during the early stage of isothermal annealing at 793 K. A theoretical function based on a model of spherical PbTe nanocrystals surrounded by a Pb and Te depleted shell fits well to all experimental curves. The time dependences of the nanocrystal radius and size of the depleted shell agree with the prediction of the theory of nucleation and growth by the classical mechanism of atomic diffusion.     

Search for the scalar top quark in pp collisions at square root[s] = 1.8 TeV

We have performed a search for scalar top quark (stop) pair production in the inclusive electron-muon-missing transverse energy final state, using a sample of pp events corresponding to 108.3 pb(-1) of data collected with the D0 detector at Fermilab. The search is done in the framework of the minimal supersymmetric standard model assuming that the sneutrino is the lightest supersymmetric particle. For the dominant decays of the lightest stop, t-->b chi+1 and t-->blnu, no evidence for signal is found. We derive cross-section limits as a function of stop ( t ), chargino ( chi+1), and sneutrino ( nu) masses.